HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 66653412, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Fluorobenzylamine | HCID 67326 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | HCID 66653630 | HCID 66653630 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 66653412 | HCID 66653412 | 94.7% |
Reaction Steps
2.14 g (7.2 mmol) of triphosgene are added, at ambient temperature under an inert atmosphere, to 2.58 g (6 mmol) of methyl 2-amino-5-({1-[3-(methoxycarbonyl)phenyl]imidazo[1,5-a]pyridin-3-yl}carbonyl)benzoate in 50 ml of dioxane. After refluxing for 7 hours, 2.25 g (18 mmol) of 4-fluorobenzylamine and 1.82 g (18 mmol) of triethylamine are added at ambient temperature. The reaction medium is refluxed for 3 hours and then concentrated under reduced pressure. The residue is triturated from water. After filtration, the solid is rinsed with methanol and then dried under reduced pressure at 40° C. overnight. 3.3 g of a yellow solid are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08759344B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-d1c8637ac9d44738a2648cb1947edff8 |
| Source note | uspto-grants-2014_06 |